Electronic Supplementary Material (ESI) for ChemComm. This journal is © The Royal Society of Chemistry 2020 Supporting Information Direct cyclohexanone oxime synthesis via oxidation-oximization of cyclohexane with ammonium acetate Ling Peng, Chan Liu, Na Li, Wenzhou Zhong*, Liqiu Mao*, Steven Robert Kirk and Dulin Yin National & Local United Engineering Laboratory for New Petrochemical Materials & Fine Utilization of Resources, Key Laboratory of Chemical Biology Traditional Chinese Medicine Research Ministry of Education, College of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, PR China *Corresponding authors: Wenzhou Zhong and Liqiu Mao Fax: +86-731-88872531; Tel.: +86-731-88872576 E-mail:
[email protected] (W. Zhou);
[email protected] (L. Mao) 1. Experimental 1.1 Catalyst preparation The hollow-structured TS-1 was synthesized under hydrothermal condition by a dissolution- recrystallization process in tetrapropylammonium hydroxide (TPAOH) solution.1 First, tetraethyl orthosilicate (TEOS), titanium butoxide (TBOT), TPAOH solution and distilled deionized water were mixed in a 1:0.01:0.4:40 molar ratio forming a clear solution, which was hydrolyzed for 2 h at 60 oC. The obtained gel was transferred to a Teflon-lined stainless steel autoclave and crystallized at 170 oC for 3 days. The white solid was filtrated and washed with large amounts of deionized water and dried at 120 oC for 24 h, followed by calcination at 500 oC for 10 h to remove the residual structure directing reagent. Secondly, the obtained solid TS-1 was treated with H2SO4 solution (a weight ratio of the previous calcined TS-1:H2SO4:water=10:1.2:140), and the acid- treated solid TS-1 was dispersed in TPAOH solution (a weight ratio of molecular sieve: TPAOH: water=10:1.5:125).